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Production and use of octafluoropropane

a technology of octafluoropropane and octafluoropropane, which is applied in the field of production and use of octafluoropropane, can solve the problems of reducing the yield and selectivity of the objective octafluoropropane, unable to obtain high-purity octafluoropropane, and difficult production of high-purity octafluoroprop

Inactive Publication Date: 2004-04-13
SHOWA DENKO KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention provides a method for producing high-purity octafluoropropane, which is a useful gas for the production of semiconductor devices. The method involves a two-step process involving the reaction of hexafluoropropene with hydrogen fluoride in a gas phase at a temperature of 150 to 450 degrees Celsius in the presence of a fluorination catalyst to obtain 2H-heptafluoropropane, followed by the reaction of 2H-heptafluoropropane with fluorine gas in a gas phase at a temperature of 250 to 550 degrees Celsius in the absence of a catalyst to obtain octafluoropropane. The resulting octafluoropropane has a high purity of 99.999 vol% or more, with a low content of compounds having a chlorine atom within the molecule and cyclic compounds. The invention also provides an octafluoropropane product with a high purity of 99.9995 vol% or more. The method and product of the invention can be used in various processes for producing semiconductor devices.

Problems solved by technology

However, in these methods, by-products such as tetrafluoromethane (CF.sub.4) and hexafluoroethane (C.sub.2 F.sub.6) are produced due to cleavage, C.sub.6 F.sub.12 and C.sub.6 F.sub.14 are produced due to radical addition, and a 4-membered ring is produced due to cyclization addition, for example, and as a result, the yield of and selectivity for the objective octafluoropropane decrease.
Furthermore, some compounds in these impurities are difficult to separate by distillation and, in turn, high-purity octafluoropropane can hardly be obtained.
Particularly, in the case of using hexafluoropropene as the starting material, chloropentafluoroethane (CFC-115) contained as an impurity scarcely reacts with fluorine gas and mostly remains in the objective octafluoropropane and since this impurity compound can hardly be separated by distillation, due to the similar boiling points, production of high-purity octafluoropropane is difficult.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

Into an Inconel 600-type reactor having an inner diameter of 1 inch and a length of 1 m, 100 ml of the catalyst, prepared according to the method described in the above Production of Fluorination Catalyst, was filled, and the temperature was elevated to 400.degree. C. while passing nitrogen therethrough. Thereto, hydrogen fluoride was fed at 6.32 NL / hr and then the gas mainly comprising hexafluoropropene as described in Starting Material Example 1 was fed at 3.24 NL / hr. By stopping the feeding of nitrogen gas, the reaction was initiated. After 2 hours, the discharged gas was washed with an aqueous potassium hydroxide solution to remove the acid content and thereafter, the gas composition was analyzed by gas chromatography and, as a result, a gas having the composition shown in Table 5 was obtained.

The gas after the removal of acid content was collected under cooling using a cylinder container and distillation-purified to remove low boiling fractions and high boiling fractions by a k...

example 2

Using the gas mainly comprising 2H-heptafluoropropane after the distillation obtained in Example 1, a direct fluorination reaction with fluorine gas was performed.

A nickel reactor having an inner diameter of 20.6 mm.phi. and a length of 500 mm (using heating by an electric heater; the reactor had been subjected to a passivation treatment with fluorine gas at a temperature of 500.degree. C.) was heated to a temperature of 400.degree. C. while passing nitrogen gas at 20 NL / hr.

Then, hydrogen fluoride (diluting gas) was fed at 60 NL / hr through two branches and, into one gas flow, the gas mainly comprising 2H-heptafluoropropane was fed at 3.24 NL / hr. Thereafter, fluorine gas was fed into another gas flow of hydrogen fluoride at 3.55 NL / hr, the feeding of nitrogen gas was stopped, and the direct fluorination reaction was performed. After 3 hours, the reaction product gas was washed with an aqueous potassium hydroxide solution and an aqueous potassium iodide solution, analyzed on hydrogen ...

example 3

Into a nickel reactor having an inner diameter of 20.6 mm.phi. and a length of 500 mm, the outlet gas containing unreacted fluorine gas obtained after the direct fluorination reaction in Example 2 was introduced. The gas composition was such that the hydrogen fluoride flow was 62.82 NL / hr, the organic material flow was 3.16 NL / hr and the unreacted fluorine gas flow was about 0.26 NL / hr. The reactor temperature was elevated to 390.degree. C., trifluoromethane as hydrofluorocarbon was fed at about 0.286 NL / hr from the reactor inlet, and unreacted fluorine and organic material composition were analyzed by titration and gas chromatography. The amount of unreacted fluorine gas in the outlet gas after the reaction with trifluoromethane was 50 ppm or less, and the outlet gas had the composition shown in Table 9.

Subsequently, the outlet gas after the removal of remaining fluorine gas was washed with an aqueous potassium hydroxide solution to remove hydrogen fluoride. The gas after the remov...

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Abstract

Octafluoropropane is produced by a process comprising a step (1) of reacting hexafluoropropene with hydrogen fluoride in a gas phase at a temperature of from 150 to 450° C. in the presence of a fluorination catalyst to obtain 2H-heptafluoropropane and a step (2) of reacting 2H-heptafluoropropane obtained in step (1) with fluorine gas in a gas phase at a temperature of from 250 to 500° C. in the absence of a catalyst to obtain octafluoropropane. High-purity octafluoropropane is obtained which can be used in a process for producing a semiconductor device.

Description

The present invention relates to a process for producing octafluoropropane, an octafluoropropane product, and uses thereof.Octafluoropropane is used, for example, as a dry-etching or cleaning gas in the process for producing a semiconductor device. With respect to the production methods thereof, the following methods are known:(1) a method of performing a direct fluorination reaction between hexafluoropropene and fluorine gas (see, Japanese Examined Patent Publication No. 62-61572 (JP-B-62-61572)),(2) a method of performing an electrolytic fluorination of hexafluoropropene in hydrogen fluoride (see, Japanese Examined Patent Publication No. 62-61115 (JP-B-62-61115)),(3) a method of reacting hexafluoropropene with fluorine in the presence of a catalyst (see, Japanese Examined Patent Publication No. 1-45455 (JP-B-1-45455)), and(4) a method of reacting hexafluoropropene with a high-order metal fluoride (see, Japanese Examined Patent Publication No. 62-54777 (JP-B-62-54777)).However, in ...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): C07C17/10C07C19/00C07C17/38C07C17/383C07C17/21C07C17/087C07C17/00C07C19/08C07C17/20
CPCC07C17/087C07C17/10C07C17/206C07C17/21C07C17/38C07C17/383C07C19/08
Inventor OHNO, HIROMOTOOHI, TOSHIO
Owner SHOWA DENKO KK
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